CN102368992B - Porous, dissolvable solid substrate and surface resident inorganic particulate perfume complexes - Google Patents

Porous, dissolvable solid substrate and surface resident inorganic particulate perfume complexes Download PDF

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CN102368992B
CN102368992B CN200980148931.3A CN200980148931A CN102368992B CN 102368992 B CN102368992 B CN 102368992B CN 200980148931 A CN200980148931 A CN 200980148931A CN 102368992 B CN102368992 B CN 102368992B
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solid substrates
dissolvable solid
approximately
spice
personal care
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CN102368992A (en
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罗伯特.W.格伦
凯西.M.考夫曼
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Procter and Gamble Ltd
Procter and Gamble Co
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25Silicon; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/463Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8129Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers or esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers, e.g. polyvinylmethylether
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q13/00Formulations or additives for perfume preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

Abstract

The present invention relates to personal care compositions, especially those personal care compositions in the form of a personal care article that is a porous dissolvable solid substrate. The porous dissolvable solid substrate has a surface resident coating comprising an inorganic particulate perfume complex that can provide a consumer benefit.

Description

Dissolvable solid substrates and surperficial resident inorganic particulate perfume complex
Invention field
The present invention relates to personal care composition, those personal care compositions of personal nursing beneficial effect are especially provided with goods form, described goods comprise dissolvable solid substrates and surperficial resident inorganic particulate perfume complex.
Background of invention
Personal care composition is sold as fluid product traditionally.These liquid personal care products comprise a large amount of water conventionally in formula.Because consumer expects fragrant personal care product conventionally, except being liquid, many personal care products also comprise spice.Yet because water is present in personal care product, comprising of spice is limited to dissolubility or the emulsifying in moisture amphiphile aggregation (micelle, liquid crystal etc.).Therefore, the perfume molecules quilt " collection " of signal portion is in these moisture aggregations, this can limit perfume delivery to the effect (that is, the strong degree of lower spice) in consumer nostril and be delivered to the effect of target cutin substrate (that is, skin and hair) at product between the operating period.In addition, the selection of spice is limited to those (that is, the fragrance of product and packing identical and experience during use unique spice) of sending single scent experience to consumer, and gets rid of sending of the spice that is activated by water during use.
Therefore, target of the present invention is to provide in consumer and can more effectively sends the personal care product of spice between the operating period.Another target of the present invention is to provide the personal care product who sends spice, and described spice can be activated by water, that is, discharge by the maximum fragrance triggering during use by add water to product.The additional target of the present invention is to provide can not only send the first spice, and sends the personal care product of the second spice, causes the eruption for the second time of the fragrance that is activated by water during use.For example, described personal care product can have a kind of fragrance before being combined with water, and after being exposed to water, and described personal care product can have the eruption of fragrance for the second time of the second fragrance and/or identical initial spice.
The further target of the present invention is to provide the more spice of high-load is provided in personal care product.
Summary of the invention
The present invention has met aforementioned needs.The present invention provides dissolvable solid substrates with the form of unit dose personal care product, described goods can facilitate and be dissolved in quickly on consumer's palm with reconstituted liquid personal care composition, when being easy to be applied on hair, before using and between the operating period, provide the fragrance of consumer's expectation.
, comprise: (i) dissolvable solid substrates, described substrate comprises: approximately 10% to approximately 75% surfactant; Approximately 10% to approximately 50% water-soluble polymer; Approximately 1% to approximately 30% plasticizer; (ii) surperficial resident coating, described coating comprises one or more inorganic particulate perfume complex of approximately 10% to approximately 100%; The ratio of inorganic particle and spice approximately 0.5: 1 to approximately 19: 1 in complex wherein.
Method for the preparation of personal care product, described method comprises the resident coating in surface is administered on dissolvable solid substrates, the inorganic particulate perfume complex that described coating comprises powder type, described substrate comprises approximately 10% to approximately 75% surfactant, approximately 10% to approximately 50% water-soluble polymer and approximately 1% to approximately 30% plasticizer.
Method for the preparation of personal care product, described method comprises: preparation process mixture, described mixture comprises approximately 10% to approximately 75% surfactant, and their combination, approximately 5% to approximately 35% water-soluble polymer and approximately 0.5% to approximately 20% plasticizer; By gas is incorporated into process mixture, process mixture is inflated, to form the wet mix of filling gas; Described wet mix of filling gas is shaped to the shape of one or more expectations; Described in dry, filled the wet mix of gas to form dissolvable solid substrates; And the resident coating in surface of the inorganic particulate perfume complex that comprises powder type is administered on described dissolvable solid substrates.
Summary of drawings
Although this description by particularly point out and clearly claimed claim of the present invention draw a conclusion, it is believed that by the explanation of following embodiment and contrast accompanying drawing and can understand better the present invention, the same reference numbers in figure represents identical element, wherein
Fig. 1 is the schematic diagram of dissolvable solid substrates and surperficial resident inorganic particulate perfume complex;
Fig. 2 is the schematic diagram of the resident inorganic particulate perfume composite layer of two dissolvable solid substrates and the surface between two substrate;
Fig. 3 A and 3B are the dissolvable solid substrates of depression and the schematic diagram of the resident inorganic particulate perfume complex of pit inner surface;
Fig. 4 is for folding to seal the schematic diagram of the dissolvable solid substrates of surperficial resident inorganic particulate perfume complex;
Fig. 5 be dissolvable solid substrates micro--CT 3-D image; With
Fig. 6 is the cross section SEM image of the top-middle part-bottom laminated of dissolvable solid substrates.
Detailed Description Of The Invention
In all embodiments of the present invention, unless stated otherwise, all percentage ratio is all by the weighing scale of described total composition.Unless stated otherwise, all ratios is weight rate.All scopes include end value interior and can merge.Number of significant digit represents neither to limit indicated amount and does not also limit certainty of measurement.Unless specifically indicated in addition, all umerical amounts are all understood to be modified by word " approximately ".Except as otherwise noted, all measurements are all understood to be to carry out under 25 ℃ and environmental condition, and wherein " environmental condition " refers to the condition under approximately one atmospheric pressure and approximately 50% relative humidity.Except as otherwise noted, all above-mentioned weight relevant to ingredients listed is the content based on active substance all, and do not comprise carrier or the by-product in the raw material that may be included in commercially available acquisition.
i. definition
As used herein, term " personal care composition " refers to and can be administered on mammalian hair and skin and without the compositions of unsuitable inadvisable effect.
As used herein, term " inorganic particulate perfume complex " refers to that spice is compounded in the releasable matrix of the water consisting of particle form inorganic material.
As used herein, term " surperficial resident inorganic particulate perfume complex " refers to that the resident coating in the surface that comprises inorganic particulate perfume complex, described complex are absorbed into the consolidate/aerosphere face of dissolvable solid substrates at least partly.The resident coating in surface of gained product stock life period ,Bing consumer between the operating period personal care product be placed in before contacting with water and minimize the Physical interaction between inorganic particulate perfume complex and solubility porosu solid main body.
As used herein, " personal care product " refer to and comprise surfactant, water-soluble polymer and plasticizer, together with the dissolvable solid substrates of the resident coating in surface of inorganic particulate perfume complex.Personal care product as herein described can be known as " goods ".
As used herein, " solubility " refers to that dissolvable solid substrates has the dissolution rate that meets manual dissolving method test as herein described.
As used herein, " dissolvable solid substrates " refers to that the solid that comprises polymer that defines space or abscess network is communicated with substrate, and described space or abscess comprise the gas in ambient atmosphere, are generally air.The interconnectivity of described structure can be long-pending by celestial body, structural model index (SMI) or perforate percentage composition are described.
iI. personal care product
Personal care product of the present invention via foaming/cleaning product by more effectively sending at consumer's operating period chien shih spice and the release ,Xiang consumer of the spice of water activation sends unique spice/spice and experiences.The spice of described water activation can comprise secondary spice, make described personal care product can before contacting with water, there is a kind of fragrance, and after being exposed to water, the fragrance for the second time that described personal care product can have the second fragrance and/or identical initial spice discharges.
This realizes by mix the resident coating in the surface that comprises inorganic particulate perfume complex on dissolvable solid substrates.Can use any suitable application process to use the resident coating in this surface, described coating is adsorbed at least part of consolidate/aerosphere face of dissolvable solid substrates.In one embodiment, the form that the resident coating in surface that comprises inorganic particulate perfume complex is powder coating, described coating is administered to the surface of dissolvable solid substrates to form personal care product.
Conventionally, spice by spice dissolving or the emulsifying in stable amphiphile aggregation (as micelle, liquid crystal etc.) from liquid, aqueous consumer goods, send.This can cause spice in the nostril of product operating period Jian Xiang consumer (that is, the strong degree of lower spice) with to more inefficient the sending of target cutin substrate (that is, skin and hair).This is attributable to " collection " of described perfume molecules in stable moisture amphiphile aggregation, this is at product between the operating period, can hinder the diffusion to water/air and water/matrix interface by water of hydrophobicity perfume molecules, therefore reduce perfume molecules to the delivery efficiency of the target that is intended to reach (consumer nostril and cutin substrate), even cause the waste (" swash of wave is to gutter ") of more substantial perfume molecules.Although this still can occur in this creative personal care product, but when described personal care product is prepared according to the present invention and/or is used, because they were at once dissolved in the water before being administered to hair or skin, this physics " collection " interacts and has been minimized.
The present invention also guarantees sending of the spice that is activated by water, that is, during use by adding water to product, the release of spice is triggered by maximum.The generation of this phenomenon is that water is releasable owing to inorganic particulate perfume complex of the present invention, that is, when described personal care product is dissolved in water, described inorganic particle dissolves, and spice physics discharges or is free thereupon.
During product is by consumer's experience, the present invention guarantees that the first spice and the second spice sends separately and optionally in addition.For example, described personal care product can have a kind of fragrance before being combined with water, and after being exposed to water, and described personal care product can have the stronger eruption of fragrance for the second time of the second fragrance and/or identical initial spice.This can be by the second spice is incorporated in described inorganic particulate perfume complex and is realized, and described the second spice has and the distinct fragrance of the first spice.Alternatively, can in inorganic particulate perfume complex, use identical spice, but when personal care product dissolves, guarantee the strong degree that spice is stronger.
a. dissolvable solid substrates
Dissolvable solid substrates comprises surfactant, water-soluble polymer and plasticizer.Can prepare dissolvable solid substrates can facilitate it and is promptly dissolved in the palm of consumer and obtains liquid personal care composition.Once dissolve, this personal care composition can be similar to the mode of conventional liquid personal care composition and use, that is, be administered on scalp, hair and/or health.Dissolvable solid substrates has maximum pore wall thickness.Described dissolvable solid substrates has about 0.02mm to about 0.15mm, about 0.025mm is to about 0.12mm in one embodiment, about 0.03mm is to about 0.09mm in another embodiment, and in another embodiment about 0.035mm to the pore wall thickness of about 0.06mm.Described dissolvable solid substrates has interconnectivity between the abscess of minimum degree, and this is long-pending by celestial body, structural model index (SMI) and perforate percentage composition quantize.Described dissolvable solid substrates has about 1mm 3to about 90mm 3, about 1.5mm in one embodiment 3to about 60mm 3, about 2mm in another embodiment 3to about 30mm 3, and about 2.5mm in another embodiment 3to about 15mm 3celestial body long-pending.Described dissolvable solid substrates has approximately 0.0 to approximately 3.0 non-negative structural model index, in one embodiment, and approximately 0.5 to approximately 2.75, and in another embodiment approximately 1.0 to approximately 2.50.Described dissolvable solid substrates has approximately 80% to 100% perforate percentage composition, and in one embodiment approximately 85% to approximately 97.5%, and in another embodiment approximately 90% to approximately 95%.Described dissolvable solid substrates also has minimum specific surface area.Described dissolvable solid substrates has about 0.03m 2/ g is to about 0.25m 2/ g, in one embodiment about 0.035m 2/ g is to about 0.22m 2/ g, in another embodiment about 0.04m 2/ g is to about 0.19m 2/ g, and about 0.045m in another embodiment 2/ g is to about 0.16m 2the specific surface area of/g.Described dissolvable solid substrates has about 125g/m 2to approximately 3,000g/m 2basic weight, about 300g/m in one embodiment 2to approximately 2,500g/m 2, about 400g/m in another embodiment 2to approximately 2,000g/m 2, about 500g/m in another embodiment 2to approximately 1,500g/m 2, and about 600g/m in another embodiment 2to approximately 1,200g/m 2, and in another embodiment approximately 700 to approximately 1,000g/m 2.Described dissolvable solid substrates has about 0.03g/cm 3to about 0.40g/cm 3density of solid, about 0.05g/cm in one embodiment 3to about 0.35g/cm 3, about 0.08g/cm in another embodiment 3to about 0.30g/cm 3, about 0.10g/cm in another embodiment 3to about 0.25g/cm 3, and about 0.12g/cm in another embodiment 3to about 0.20g/cm 3.
In one embodiment, dissolvable solid substrates of the present invention is the flat flexible substrate of pad, bar or ribbon form, and measure according to method below, there is about 0.5mm to about 10mm, about 1mm is to about 9mm in one embodiment, about 2mm is to about 8mm in another embodiment, and in another embodiment about 3mm to the thickness of about 7mm.
1. surfactant
In the relevant operation instruction of Yu consumer, dissolvable solid substrates of the present invention can be and bubbles or bubble-tight.Described solubility porous matrix comprise at least one surfactant as processing aid with in the stable foam solid of dry (solidifying) front generation, and the in the situation that of foaming substrate, surfactant also can be taken on dual-use function as foaming agent and/or cleaning agent.
a. dissolvable solid substrates bubbles
For bubble and/or the foaming dissolvable solid substrates of clean object by described personal care product weighing scale, comprise approximately 10% to approximately 75%, in one embodiment approximately 30% to approximately 70%, and approximately 40% to approximately 65% surfactant in another embodiment; Wherein said surfactant comprises that one or more derive from the surfactant of I class, wherein I class comprises the anion surfactant that is applicable to hair-care or other personal care composition, and choose any one kind of them or the multiple surfactant that derives from II class, wherein II class comprises the freely surfactant that is applicable to hair-care or other personal care composition of the group of following composition of choosing: both sexes, zwitterionic and their combination; Wherein the ratio of I class and II class surfactant is approximately 100: 0 to approximately 30: 70.In another embodiment of the invention, the ratio of I class and II class surfactant approximately 85: 15 to approximately 40: 60.In another embodiment of the invention, the ratio of I class and II class surfactant approximately 70: 30 to approximately 55: 45.
The limiting examples of anion surfactant is described in United States Patent (USP) 2,486, in 921,2,486,922 and 2,396,278.The group of the following composition of the optional freedom of described anion surfactant: alkyl sulfate and alkyl ether sulfate, Sulfated monoglyceride, the alkene of sulfonation, alkylaryl sulfonates, uncle or secondary alkyl sulfonate, alkyl sulfosuccinate, acid taurate, acid isethionate, alkyl glycerol ether sulfonate, sulfonation methyl ester, alpha-sulfonated fatty acid, alkylphosphonic, acyl glutamate, acyl sarcosinates, alkyl lactate, anionic fluorosurfactants, sodium lauroyl glutamate, and their combination.
The limiting examples of suitable zwitterionic or amphoteric surfactant is described in United States Patent (USP) 5,104,646 (authorizing the people such as Bolich Jr.) and 5,106,609 (authorizing the people such as Bolich Jr.).
Additional suitable I class and II class surfactant comprise and are disclosed in United States Patent (USP) publication application No.61/120, those in 765 and the Detergents and Emulsifiers that is disclosed in McCutcheon, North America version (1986), Allured Publishing Corp.; The Functional Materials of McCutcheon, North America version (1992), those surfactants in Allured Publishing Corp.; Disclose 3,929 with United States Patent (USP), in 678 (authorizing the people such as Laughlin).The limiting examples of the surfactant that other is suitable is included in United States serial 61/120,790.
b. non-foaming dissolvable solid substrates
Described non-foaming dissolvable solid substrates by described personal care product weighing scale, comprises approximately 10% to approximately 75%, and in another embodiment approximately 15% to approximately 60%, and approximately 20% to approximately 50% surfactant in another embodiment; Wherein said surfactant comprises the surfactant that one or more are following.
(i) anion surfactant
If dissolvable solid substrates of the present invention is bubble-tight, the anion surfactant that substrate can comprise high-load 10% (or being less than 10%) so with when the stable foam solid of preparation mainly as processing aid.In addition, non-ionic surface active agent can be combined with anion surfactant to reach the surfactant level that produces stable foam solid before dry.
(ii) non-ionic surface active agent
In one embodiment, comprise non-ionic surface active agent as the processing aid in preparing stable dissolvable solid substrates.The ionic surfactant pack being applicable in the present invention is drawn together those that describe in " Detergents and Emulsifiers " North America version (1986, Allured Publishing Corp.) of McCutcheon and " Functional Materials " the North America version (1992) of McCutcheon.The ionic surfactant pack being applicable in personal care composition of the present invention is drawn together but is not limited to, polyoxyethylenated alkylphenol, polyoxyethylenated alcohol, polyoxyethylene polypropylene glycol, alkanoic acid glyceride, alkanoic acid polyglycerin ester, alkanoic acid propylene glycol ester, alkanoic acid sorbitol ester, alkanoic acid polyoxyethylene sorbitol ester, alkanoic acid polyoxyethylene glycol ester, polyoxyethylene alkanoic acid, alkanolamide, N-alkyl pyrrolidone, alkyl polyglucoside, alkyl polyglucoside, alkyl amine oxide and polyoxyethylene siloxanes.
(iii) polymeric surfactant
Polymeric surfactant can be equally in dissolvable solid substrates of the present invention preparation, separately or with ion and/or the nonionic surfactant combinations surfactant as processing aid.The polymeric surfactant being applicable in personal care composition of the present invention includes but not limited to, the block copolymer of block copolymer, oxirane and expoxy propane of oxirane and fatty alkyl residue is, the cellulose of the polyacrylate of hydrophobically modified, hydrophobically modified, polyether silicon, silicone copolyol ester, polydimethylsiloxane bi-quaternary ammonium salt and the altogether amino/polyether silicone of modification.
2. water-soluble polymer (" polymer architecture agent ")
Described dissolvable solid substrates comprises the water-soluble polymer as structural agent.As used herein, the enough broad sense of term " water-soluble polymer ", comprises water solublity and aqueous dispersion polymers, and is defined as, at 25 ℃, measure, in water, dissolubility is at least about the polymer of 0.1 grams per liter (g/L).In some embodiments, at 25 ℃, measure, described polymer has approximately 0.1 grams per liter (g/L) to dissolubility in the water of approximately 500 grams per liters (g/L).(this represents to obtain macroscopically isotropic or transparent coloured or colourless solution).For the preparation of the polymer of these solids, can be derived from synthetic or natural, and can be via chemical reaction modification.They can film forming or can not film forming.These polymer should be that physiology is upper acceptable, and they should be compatible with skin, mucosa, hair and scalp.
By described dissolvable solid substrates weighing scale, described one or more water-soluble polymers can approximately 10% to approximately 50% exist, in one embodiment by described dissolvable solid substrates weighing scale, approximately 15% to approximately 40%, and in another embodiment by described dissolvable solid substrates weighing scale, approximately 20% to approximately 30%.
Select one or more water-soluble polymers of the present invention, the weight average molecular weight that makes them is approximately 40,000 to approximately 500,000, be approximately 50,000 to approximately 400,000 in one embodiment, be approximately 60 in another embodiment, 000 to approximately 300,000, and be approximately 70 in another embodiment, 000 to approximately 200,000.By the mean molecule quantity of every kind of polymer raw material is multiplied by they separately by the relative weight percentage ratio of contained total polymer weight in dissolvable solid substrates, add and calculate weight average molecular weight.
In one embodiment, by solution weight, select at least one in one or more water-soluble polymers to make approximately 2% described water-soluble polymer provide the viscosity of approximately 4 centipoises to approximately 80 centipoises at 20 ℃; In an alternative embodiment, approximately 5 centipoises are to approximately 70 centipoises; And approximately 6 centipoises are to approximately 60 centipoises in another embodiment.
Water-soluble polymer of the present invention can include but not limited to synthetic polymer, as be described in United States Patent (USP) serial number 61/120, in 786, comprise the polymer derived from polyacrylic monomer, carboxylic monomer as unsaturated in ethylenic and ethylenically unsaturated monomers, as be described in US 5,582,786 and EP-A-397410 in.Suitable water-soluble polymer also can be selected from natural source polymer, comprises those of plant source, and the example is described in United States Patent (USP) serial number 61/120,786.The natural polymer of modification also can be used as the water-soluble polymer in the present invention, and comprises in United States Patent (USP) serial number 61/120,786.In one embodiment, water-soluble polymer of the present invention comprises polyvinyl alcohol, polyacrylate, polymethacrylates, acrylic acid and methyl acrylate copolymer, polyvinylpyrrolidone, polyalkylene oxide, starch and starch derivatives, Pullulan, colloid, hydroxypropyl emthylcellulose, methylcellulose and carboxymethyl cellulose.In another embodiment, water-soluble polymer of the present invention comprises polyvinyl alcohol and hydroxypropyl emthylcellulose.Suitable polyvinyl alcohol comprises with trade name
Figure BDA0000066753880000081
derive from those of Celanese Corporation (Dallas, TX).Suitable hydroxypropyl emthylcellulose comprises with trade name
Figure BDA0000066753880000091
derive from those of Dow Chemical Company (Midland, MI).
In specific embodiments, above-mentioned water-soluble polymer can be certain amount with as any single starch of packing material or starch combination blend, to reduce required water-soluble polymer total content, as long as this contributes to provide the personal care product with desired structure and physical/chemical properties as described herein.
In the case, with respect to dissolvable solid substrates gross weight, the combined wt percentages of water-soluble polymer and starch-based material is generally approximately 10% to approximately 50%, in one embodiment approximately 15% to approximately 40%, and in specific embodiments approximately 20% to approximately 30% scope.The weight ratio of water-soluble polymer and starch-based material generally can be at approximately 1: 10 to approximately 10: 1, approximately 1: 8 to approximately 8: 1 in one embodiment, approximately 1: 7 to approximately 7: 1 in another embodiment, and in another embodiment approximately 6: 1 to about 1: 6 scope.
The typical case source of starch-based material can comprise cereal, tuber, root, beans and fruit.Natural origin can comprise Semen Maydis, Semen Pisi sativi, Rhizoma Solani tuber osi, Fructus Musae, Fructus Hordei Vulgaris, Semen Tritici aestivi, rice, sago, Amaranthus, Maninot esculenta crantz., Rhizoma Marantae arundinaceae, Canna generalis Bailey, Sorghum vulgare Pers. and their waxiness or taka-diastase kind.Starch-based material also can comprise the native starch that uses any modified form modification known in the art, comprises and is described in those in United States Patent (USP) serial number 61/120,786.
3. plasticizer
Dissolvable solid substrates of the present invention comprises the water-soluble plasticizer being applicable in personal care composition.In one embodiment, by described dissolvable solid substrates weighing scale, one or more plasticizers can approximately 1% to approximately 30% exist; In another embodiment, approximately 3% to approximately 25%; In another embodiment, approximately 5% to approximately 20%, and in another embodiment, approximately 8% to approximately 15%.Suitable plasticizer limiting examples comprises polyhydric alcohol, polyol, polybasic carboxylic acid, polyester and dimethicone copolyol.The example of available polyhydric alcohol includes but not limited to, glycerol, two glycerol, propylene glycol, ethylene glycol, butanediol, pentanediol, cyclohexanedimethanol, hexanediol, Polyethylene Glycol (200-600), sugar alcohol, as sorbitol, mannitol, lactose and other monobasic and polynary low-molecular-weight alcohol (as, C2-C8 alcohol); Monosaccharide, disaccharide and oligosaccharides, as fructose, glucose, sucrose, maltose, lactose and senior fructose corn-syrup solids and ascorbic acid.Can be used for the suitable example of polybasic carboxylic acid is herein disclosed in United States Patent (USP) serial number 61/120,786.
In one embodiment, plasticizer comprises glycerol or propylene glycol, and their combination.European patent number EP283165B1 discloses other suitable plasticizer, comprises glycerol derivatives, as propoxylated glycerol.
4. optional member
Dissolvable solid substrates also can comprise and becomes known for or can be used for other optional member in personal care composition, precondition is that examples of such optional materials is compatible with selected base substance described herein, or can suitably weaken the performance of personal care composition.
Examples of such optional composition is generally those materials for cosmetics by approval most, and is described in handbook, as CTFA Cosmetic Ingredient Handbook, second edition, The Cosmetic, Toiletries, and Perfume Association, Inc.1988,1992.The example of examples of such optional composition is disclosed in the United States Patent (USP) serial number 12/361,634,10/392422 of submitting on March 18th, 2003; Announce in 2003/0215522A1 with the U.S. on November 20th, 2003.
Other optional member comprises organic solvent, especially as polymer architecture agent and as the water miscible solvent and the cosolvent that are dried promoter.The example of suitable organic solvent is disclosed in United States Patent (USP) serial number 12/361,634.Other optional member comprises: latex or emulsion polymer, the thickening agent such as water-soluble polymer, clay, silicon dioxide, glycol distearate, deposition aid, comprise that coacervate forms component.Additional optional composition comprises anti-dandruff active, includes but not limited to OMADINE, selenium sulfide and be disclosed in the U.S. announce those active substances in 2003/0215522A1.
B. the resident coating in surface that comprises inorganic particulate perfume complex
In one embodiment, the high surf zone " support " (3-D " pillar " network) that dissolvable solid substrates provides continuously and easily obtains to the resident coating in the surface that comprises inorganic particulate perfume complex, described complex is absorbed or scatters and forms the coating that high surf zone is thin.This position is placed in coating the position that directly contacts during use water, perfume releasing from encapsulated.
In one embodiment, surperficial resident coating comprises one or more inorganic particulate perfume complex of approximately 10% to approximately 100%; In another embodiment, approximately 25% to approximately 100%, in another embodiment approximately 40% to approximately 100%.In one embodiment, dissolvable solid substrates is approximately 110: 1 to approximately 0.5: 1 with the ratio of the resident coating in surface that comprises inorganic particulate perfume complex, approximately 20: 1 to approximately 1: 1 in another embodiment, approximately 10: 1 to approximately 1.5: 1 in another embodiment, and approximately 7: 1 to approximately 3: 1 in another embodiment.
inorganic particulate perfume complex
One or more first and/or second spice can be by compound to the releasable matrix of water consisting of particle form inorganic material.In one embodiment, in complex, the ratio of inorganic particle and spice is approximately 0.5: 1 to approximately 19: 1, and approximately 0.7: 1 to approximately 6: 1 in another embodiment, and approximately 1: 1 to approximately 3: 1 in another embodiment.
Inorganic particulate perfume complex of the present invention is prepared from inorganic material, described inorganic material comprises silicon dioxide (silicon dioxide), silicate or carbonate, and wherein said silicate and carbonate is the formation of reacting with alkali (IA) metal, alkaline earth (IIA) metal or transition metal by carbonate or silicate.Be applicable to inorganic material herein and comprise calcium silicates class, amorphous carbon/silicon dioxide, calcium carbonate, magnesium carbonate, sodium aluminosilicate or zinc carbonate and their mixture.Some instantiations that can be used for silicate of the present invention and carbonate are set forth in Van Nostrand Reinhold ' s Encyclopedia of Chemistry more full and accurately, the 4th edition, 155th, (1984) in 169,556 and 849 pages, it is incorporated herein by reference.
Exist especially and synthesize version about the inorganic material of silicon dioxide and silicate.Synthetic version is by chemical reaction controlled in manufacturing process rather than use then further refining version natural, exploitation of these compounds.Can be used for the synthetic carbonate of the present invention and can derive from various suppliers, as Mallinckrodt or Whittaker, Clark and Daniels.The example that can be used for the synthetic calcium silicates class of the present invention is 250 or
Figure BDA0000066753880000112
600, derive from the example that J.M.Huber (Havre de Grace, MD) can be used for the synthetic silicon dioxide of the present invention and be
Figure BDA0000066753880000113
80,
Figure BDA0000066753880000114
110SD, Zeosyl 200, Zeofree 5161, Zeofree 5162 and
Figure BDA0000066753880000115
265, derive from equally J.M.Huber.The example that can be used for the synthetic sodium aluminosilicate of the present invention comprises
Figure BDA0000066753880000116
7, Zeolex201, Zeolex 23A and Zeolex 7A, derive from J.M.Huber equally.
Be applicable to inorganic material of the present invention and comprise synthetic calcium silicate class.In one embodiment, synthetic calcium silicate class of the present invention is
Figure BDA0000066753880000117
600, derive from J.M.Huber, it is in the news and has the oil absorption of 475cc/100g, the particle mean size of 6 microns, the BET surface area of 300 meters squared per gram and the bulk density of 8lbs/CFT.
Be applicable to multiple spice/spice that spice herein comprises any personal care product of being applicable to.
the first spice
Personal care composition of the present invention comprises the first spice, and its before using (that is, before goods contacts with water) provide that the fragrance of described goods expectation or difficulty discover/fragrance of neutrality.Dulcet the first spice can comprise any spice or chemically be suitable for topical application to skin and the spice that is applicable to personal care composition.
The concentration of the first spice in described personal care composition should provide required fragrance effectively, includes but not limited to what difficulty was discovered.In general, the concentration of dulcet main spice counts approximately 0.0% to approximately 30.0% by the weight of described solid articles, being approximately 1% to approximately 20% in one embodiment, is approximately 2% to approximately 10% in another embodiment, and is approximately 3% to approximately 8% in another embodiment.The first spice can be contained in personal care composition of the present invention as free spice.
the second spice
For the second spice conversion (as being converted to another kind from a kind of spice) is provided, the present invention's the second spice should be significantly different and completely different with the composition of the first spice, so that the habitual effect of customer service spice, and make the second spice cover the first spice completely and highlight.Alternatively, be wherein desirably in identical spice in whole goods use procedure, described the second spice is answered substantially the same and is difficult to identification with the composition of the first spice, to provide single, continuous, lasting spice to experience.
In general, by described solid articles weighing scale, personal care composition of the present invention can comprise the second spice of approximately 0.1% to approximately 30.0%, in specific embodiments approximately 1% to approximately 20%, in another embodiment approximately 2% to approximately 10%, and still in another embodiment approximately 3% to approximately 8%.
Any spice or the spice that is chemically suitable for being applied topically to skin and is applicable to personal care composition can be used as the second spice, yet it will not be included in compositions as free spice.T the second spice is by the releasable matrix of the water that is contained in surfactant-free.The group of the following composition of the optional freedom of the second spice: spice, there is boiling point and be less than the high volatile volatile spice material of approximately 250 ℃ and their mixture.This type of spice will be contained in the releasable matrix of water, and described matrix is formed by following material: capsule encapsulation material as described herein.
In one embodiment, the second spice be selected from ClogP be greater than approximately 2 and odor detection threshold be less than or equal to the humorous fragrant fragrance component of height impact of 50 parts every 1,000,000,000 parts (ppb).
According to inorganic particle complex of the present invention, be anhydrous.Yet, because process limitations, after scribing even shortly and having made, may there is remaining water.Conventionally there is water and will enter again described particle composites subsequently, for example, at duration of storage.Containing water, not only comprise water, but also comprise additional water-soluble component, as alcohol; Wetting agent, comprises polyhydric alcohol (as glycerol and propylene glycol); Activating agent, as d-pantothenylol, vitamin B 3and derivant (as nicotiamide) and plant extract; Thickening agent and antiseptic.By described encapsulated thing weighing scale, containing water, be equivalent to be no more than 20%, and by described particle composites weighing scale, can contain and have an appointment 0.001%, but be no more than approximately 20%, be no more than approximately 10%, be no more than approximately 5%, or be no more than approximately 2%.
According to inorganic particulate perfume complex of the present invention, can have approximately 1 μ m to the granularity of approximately 200 μ m, approximately 2 μ m are to approximately 100 μ m in another embodiment, and in another embodiment approximately 3 μ m to approximately 50 μ m.
The resident coating in surface is applied on dissolvable solid substrates.In one embodiment, the resident coating in described surface is fine powder form.As shown in Figure 1, in certain embodiments of the invention, described personal care product 10 comprises and is positioned at the dissolvable solid substrates 14 resident coatings 12 in the lip-deep surface of at least a portion.Should be appreciated that the resident coating 12 in described surface always can not be close to described dissolvable solid substrates 14.In certain embodiments, the resident coating 12 in described surface can be permeated dissolvable solid substrates 14 all or in part.
Alternatively, the resident coating in described surface can involved (as by double team or parcel) as described in personal care product or its parts.This type of surperficial resident coating can be by spraying, dusting, spraying, coating, surface printing (as the shape of ornament, decorative pattern or pattern with expectation), topple over, be expelled to inside, dipping or by any other suitable method, as by use depositor, sieve or powder bed.In the embodiment shown in Fig. 3 A, 3B and 4, described personal care product 10 comprises the resident coating in surface that can be positioned at below described dissolvable solid substrates surface.As shown in Figure 3 B, it is the profile of personal care product 10, and the resident coating 24 in described surface is positioned at the pit 22 of described dissolvable solid substrates 26.
Referring now to Fig. 2,, in certain embodiments, described powder is by double team between two dissolvable solid substrates, and so latter two substrate is joined together (as the water by with thin layer and/or plasticizer sealing adjacently situated surfaces or edge so that dissolvable solid substrates application pressure are to cause adhesion as described in substantially not dissolving.In this embodiment, described personal care product 10 comprises two dissolvable solid substrates 16,18, and surperficial resident coating 20 is therebetween.
Alternatively, in certain embodiments, described powder can, on a kind of personal care product that is folded to form pouch, encase described powder.As shown in Figure 4, described personal care product 10 comprises the resident coating 32 in the surface being encapsulated in folding dissolvable solid substrates 34.
The resident inorganic particulate perfume composite coating in surface of the present invention also can be given other desired attribute to personal care product, includes but not limited to the visual appearance improving.In addition, the resident inorganic particulate perfume composite coating in surface of the present invention can provide additional beneficial effect, as give anti-adhesion properties and using and minimize goods to the adhesion of the packing of product or in the situation that goods are delivered as a pile goods therein, the adhesion to other goods.
iII. the product form of personal care product
Described personal care product can be prepared to any various product form, comprise the dissolvable solid substrates together with the resident coating in described surface, the resident coating in described surface comprises inorganic particulate perfume complex, and described complex is used separately or uses with other personal nursing combination of components.No matter product form, the product form embodiment of expection comprises the personal care product of selecting and limiting herein, the combination of the resident coating in surface that described goods comprise dissolvable solid substrates and comprise inorganic particulate perfume complex.
In one embodiment, described personal care product has for one or more form that suitable size makes consumer's energy flat scraps of paper of easy to handle or mat.It can have pros, rectangular or disc-like shape, or any other suitable shape.Described paying somebody's debt and expecting repayment later can be continuous strip form, is included in the bar of sending on banded roller allotter, and unitary part providing via perforation and/or cutting mechanism is provided for it.Alternatively, described personal care product is one or more cylindrical objects, spherical object, tubular articles or any other shaped object form.
Described personal care product can comprise the surface that comprises word, sign or pattern one or more veinings, depression or pattern patterning.Because the outmost surface of described substrate comprises the part with respect to other region projection of surface, so veining substrate can be caused by matrix shape.Bossing can be caused by formed personal care product shape, for example described personal care product originally can recess or the form of waffle-like pattern form.Bossing can also be by the processing of creasing, printing coating, embossed pattern, be laminated on other layer with bossing and produce, or produced by dissolvable solid substrates self physical form.Described texturing also can be a kind of dissolvable solid substrates is laminated to the result on textured the second dissolvable solid substrates.In a particular, described personal care product available pores or groove thrust or run through the solid of described porous.
iV. preparation method
Described personal care product can be prepared by following method, and described method comprises: the polymer architecture agent that (1) preparation comprises surfactant, dissolving and the process mixture of plasticizer; (2) by gas being introduced into process mixture, inflate described process mixture to form the wet mix of filling gas; (3) described wet mix of filling gas is molded into the shape of one or more expectations; (4) wet mix of filling gas described in dry is to form dissolvable solid substrates; (5) by the resident coatings applications in the surface that comprises inorganic particulate perfume complex, powder type to described dissolvable solid substrates.
a. the preparation of process mixture
General by under the existence of water, plasticizer and other optional member, via heating, polymer architecture agent is dissolved, then cooling, prepare process mixture.This can be stirred system or be realized via any suitable continuous system by any suitable hot batch of material, and described continuous system relates to single screw rod or twin-screw extrusion, or has the heat exchanger of high shear or static agitation effect simultaneously.Can imagine any method, described polymer is finally dissolved under the existence of water, surfactant, plasticizer and other optional member, comprise the step-by-step processing by any composition built-up section premix is carried out.
Process mixture of the present invention comprises: the weighing scale by described process mixture before dry, approximately 15% to approximately 60% solid, approximately 20% to approximately 55% solid in one embodiment, approximately 25% to approximately 50% solid in another embodiment, and approximately 30% to approximately 45% solid in another embodiment; And have approximately 2, and 500cps is to approximately 150, the viscosity of 000cps, and in one embodiment approximately 5,000cps is to approximately 100,000cps, in another embodiment approximately 7,500cps is to approximately 75,000cps, and still in another embodiment, approximately 10,000cps is to approximately 60,000cps.
Solid % content be all solids, semisolid and dewater and any remarkable volatile material if the liquid component beyond low-boiling point alcohol is by the percentage by weight sum of total process mixture weighing scale.The viscosity numerical value of described process mixture is used TAInstrumentsAR500Rheometer, under the shear rate reciprocal of 1.0 seconds, at 23 ℃, with parallel-plate and 1,200 micron of gap of 4.0cm diameter, in the time of 30 seconds, measures.
b. the inflation of process mixture
The inflation of process mixture realizes by gas being incorporated into described mixture.In one embodiment, this is undertaken by mechanical mixture energy.In another embodiment, this can realize by chemical mode.Can realize inflation by any suitable machining process, described method includes but not limited to: (i) via churned mechanically autoclave inflation at intermittence, comprise planet strrier or other suitable stirred vessel, (ii) for the semicontinuous or continous way of food industry, inflate (pressurize or do not pressurize), or (iii) the dry described process mixture of spraying to form globule or the granule that filled gas, described globule or granule can be compressed, as added hot compression in mould, to form porosu solid.
Found in specific embodiments, described personal care product can make in continuous pressure aerator, and described aerator is generally used for preparing in the food industry of cotton candy.Suitable continuous pressure aerator comprises Morton agitator (Morton Machine Co. (Motherwell, Scotland)), the continuous automatic stirrer of Oakes (E.T.Oakes Corporation (Hauppauge, New York)), Fedco continuous stirred tank reactor (The Peerless Group (Sidney, and Preswhip (Hosokawa Micron Group (Osaka, Japan)) Ohio)).
Inflation also can be used CBA, by effervescent system, forms to realize (by the chemical reaction of one or more compositions, comprise and form carbon dioxide (CO by gas on the spot 2(g)).Additional may be to inflate by volatile foaming agent, as low boiling hydrocarbon or alcohol, includes but not limited to isopentane, pentane, isobutene., ethanol etc.
In one embodiment, higher than ambient temperature but lower than will cause any component do not expect, at any temperature of degraded, described premix to be preheated before gas filling technology is about to start.In one embodiment, described mixture remains on higher than approximately 40 ℃ and lower than approximately 99 ℃, in another embodiment higher than approximately 50 ℃ and lower than approximately 95 ℃, in another embodiment higher than approximately 60 ℃ and lower than approximately 90 ℃.In one embodiment, when pre-composition viscosity approximately 20 at ambient temperature, 000cps is to approximately 150, during 000cps, should be before aeration step optional laser heating.In another embodiment, during gas filling technology, apply additional heating to be dried at aeration period and to keep high temperature.This can be by by one or more surface conductivity heating, injected steam, surround or other processing mode is realized with hot bath.
In one embodiment, the moistening density range of the premix of inflation is at about 0.12g/cm 3to about 0.50g/cm 3, in scope, about 0.15g/cm in another embodiment 3to about 0.45g/cm 3, about 0.20g/cm in another embodiment 3to about 0.40g/cm 3, and about 0.25g/cm in another embodiment 3to about 0.35g/cm 3.
c. form the wet process mixture of filling gas
Described formation of filling the moistening process mixture of gas can realize by any suitable mode, to form, there is the shape of expectation or the mixture of various shape, include but not limited to that (i) deposits to the described mixture that filled gas on the mould that comprises non-interacting and non-adhering surfaces of the shape and size with expectation, described surface comprises aluminum, polytetrafluoroethylene, metal, HDPE, Merlon, neoprene, rubber, LDPE, glass etc.; (ii) the described mixture that filled gas is deposited on the hole that is imprinted on the dried particles shape starch being included in tray, be known as in addition starch mold forming technique; (iii) the described mixture that filled gas is deposited on continuous band or screen cloth, described screen cloth comprises any non-interacting and non-adhesive material, polytetrafluoroethylene, metal, HDPE, Merlon, neoprene, rubber, LDPE, glass etc., described band or screen cloth be imprinted pattern, cutting, embossing or be stored on roller subsequently.
the moistening process mixture of filling gas described in being D. dried becomes dissolvable solid substrates
Can be by any suitable device, the wet process mixture of filling gas forming is dry, described device includes but not limited to: (i) drying chamber, comprises the chamber with controllable temperature and pressure or atmospheric condition; (ii) drying baker, comprises non-convection current or the convection type drying baker with controllable temperature and optional humidity; (iii) truck storage tank exsiccator/tray dryer; (iv) multistage embedded exsiccator; (v) impact type drying baker; (vi) rotary dry case/exsiccator; (vii) embedded roaster; (viii) quick high heat transfer drying baker and exsiccator; (ix) two bellows roasters and (x) conveyer dryer, and their combination.Can adopt and not comprise cryodesiccated any suitable drying device.
Described baking temperature can be within the scope of approximately 40 ℃ to approximately 200 ℃.In one embodiment, described dry environment is heated to the temperature between 100 ℃ and 150 ℃.In another embodiment, described baking temperature is between 105 ℃ and 145 ℃.In another embodiment, described baking temperature is between 110 ℃ and 140 ℃.In another embodiment, described baking temperature is between 115 ℃ and 135 ℃.
Other suitable dry environment comprises " stereoscopic heating " technology, uses altofrequency electromagnetic field, as microwave drying and radio frequency (RF) dry.Use these technology, energy electromagnetic ground shifts through the moistening premix that filled gas, rather than by conduction or convection current.
Can be during any of above-mentioned four procedure of processings, or even after dry processing, add optional member.
e. the resident coating in surface that preparation comprises inorganic particulate perfume complex
Inorganic particulate perfume complex of the present invention can pass through multiple mixing arrangement, include but not limited to the agitator of commercially available acquisition, as two asymmetric centrifugal stirrers, vee-blender, bipyramid blender, belt blender, rotating cylinder agitator, high-shear mixer, many mechanical agitators, passive agitator (comprising static mixer and baffled passive agitator), horizontally rotate rotating cylinder agitator, rotation rotating cylinder agitator, fluid bed agitator, instantaneous fluid bed agitator (comprises Y-agitator, V-agitator, zigzag agitator etc.)/free-falling rolling type agitator etc., perfumery oil is mixed in inorganic material until described mixture is prepared for mixture uniformly.Optionally, the mixture granularity of gained can be used the granularity decline technology of commercially available acquisition, as sledge mill, impact grinding, ball milling or fluid energy mill, until obtain the particle size distribution of expectation, reduces granularity.
Alternatively, inorganic particulate perfume complex of the present invention can be dried preparation by spraying, wherein said spice disperses or is emulsifiable in the Aquo-composition that comprises inorganic material, at high shear (having optional emulsifying agent) and spray-dired one-tenth fine powder.Described optional emulsifier can comprise that the starch of Radix Acaciae senegalis, special modification or other surfactant proposing in the dry field of spraying are (referring to Flavor Encapsulation, Sara J.Risch and Gary A.Reineccius write, 9th, 45 to 54 pages (1988), it is incorporated herein by reference).
Other known method of manufacturing inorganic particle capsule encapsulation material of the present invention includes, but not limited to fluidized bed agglomeration, extrudes, cooling/method for crystallising, and the polyreaction that promotes interface with phase transfer catalyst.
Alternatively, described perfumery oil can be absorbed in inorganic nodular powder or with inorganic nodular powder and be combined, and described inorganic nodular powder is produced by multiple mechanical mixture mode (spraying is dried, mills, mill etc.) in advance.In one embodiment; with the inorganic material of pellet or granule or other solid-based form, (Qie Ru supplier provides; comprise any trace impurity component; comprise remaining solvent and plasticizer) can pass through multiple machinery; for example in dismembyator or hammer mill under the existence of spice, be milled or grind to form fine powder.
In one embodiment, the resident coating in the present invention surface can have approximately 1 μ m to the granularity of approximately 200 μ m, and approximately 2 μ m are to approximately 100 μ m in another embodiment, and in another embodiment approximately 3 μ m to approximately 50 μ m.
In some embodiments, inert filler can be in powder production and during processing to be enough to improving flow of powder characteristic and to be enough to alleviate viscosity between granule or the amount of agglomeration, being included in granular complex forms in technique, or after forming, granular complex is included, starch ocentyl succinic aluminum for example, and with trade name
Figure BDA0000066753880000181
pC derives from Akzo Nobel.During granular complex forms technique, other optional excipient as described herein or beautifying active substance can be incorporated in described powder.The powder of gained also can with other inert powder, as described herein inert material or other powder activity substance complex blend.
f. by the resident coating in the surface that comprises inorganic particulate perfume complex and described solubility porosu solid substrate combination
Any suitable application process can be used to use the resident coating in the surface that comprises inorganic particulate perfume complex to personal care product, makes it form a part for described personal care product.For example, described dissolvable solid substrates can have the surface of being clamminess, and the surface by dried soluble porous solid matrix before applying at powder to specific water content adheres on described porosu solid with the resident coating in surface that is conducive to comprise inorganic particulate perfume complex.In one embodiment, described dissolvable solid substrates is dried to approximately 0.1% to approximately 25% water content, in one embodiment approximately 3% to approximately 25%, in another embodiment approximately 5% to approximately 20%, and in another embodiment approximately 7% to approximately 15%.Alternatively, pre-dry dissolvable solid substrates surface can be formed under controlled humidity environment, before the described powder of application, reversibly absorbs specific a period of time of airborne moisture of expectation content until reach balance.In one embodiment, humidity environment is controlled in approximately 20% to approximately 85% relative humidity; Approximately 30% to approximately 75% relative humidity in another embodiment; And approximately 40% to approximately 60% relative humidity in another embodiment.
In another embodiment, described dissolvable solid substrates is placed in bag, dish, band or the rotating cylinder that comprises or be in other words exposed to described powder and stirs, rolls, brushes, shakes or shake with in batches or quantity-produced mode is used and the described powder that distributes.Other powder method of application can comprise powder sieve, electrostatic applications, triboelectrification, fluid bed, powder coated rifle, corona guns, rotating cylinder machine, electrostatic fluidized bed, electromagnetic brush and/or powder spray booth.The resident coating in surface that comprises inorganic particulate perfume complex can be applied to part or the whole region of dissolvable solid substrates outer surface, and can be applied to dress up, decorate, to form the modes such as logo, design.
v. method of testing
a. dissolution rate
Personal care product of the present invention has the dissolution rate that described personal care product is broken fast between the operating period of water application.The dissolution rate of described personal care product is determined according to following methodology.
Manual dissolving method: (if 3 to 10mm thick sheet material/mat forms, about 10 to 20 square centimeters) described personal care product (as described in this paper embodiment) is placed on the palm of wearing nitrile glove by 0.5 to 1.5g.By 7.5cm 3warm tap water (approximately 30 ℃ to approximately 35 ℃) by syringe, be promptly applied on described personal care composition.Adopt circular motion, palm is rubbed together at every turn and is wiped 2 strokes, until dissolve (30 strokes at the most).Manual solubility value is recorded as and dissolves formation number used completely, or be recorded as maximum 30 strokes.With regard to latter event, also record the not weight of dissolved material.
Personal care product of the present invention has approximately 1 to approximately 30 stroke, approximately 2 to approximately 25 strokes in one embodiment, approximately 3 to approximately 20 strokes in another embodiment, and the manual solubility value of approximately 4 to approximately 15 strokes in another embodiment.
b. thickness
Use micrometer or thickness gauge as tray frame type digital micrometer (the Mitutoyo Corporation of Mitutoyo Corporation model IDS-1012E, 965Corporate Blvd, Aurora, IL, USA60504), obtain the thickness of described personal care product and/or described dissolvable solid substrates.Described micrometer has the platen of heavily approximately 32 grams of 1 inch diameter, and it is at about 40.7phi (6.32gm/cm 2) exerting pressure under mensuration thickness.
By platen is risen, a part of sample is placed on the base under platen, reduce carefully platen to contact described sample, discharge platen, and read according to numeral, measure and take the thickness of the sample substrate that millimeter is unit, measure the thickness of personal care product and/or dissolvable solid substrates.Described sample should extend to the whole edge of described platen completely, to guarantee measuring thickness under minimum possible surface pressing, only in not flat more rigid sample situation.With regard to not exclusively flat more rigid sample, only use a part of platen contacting with sample flat part, measure the flat edge of sample.With respect to pad or bar, mostly have in cylindrical object, spherical object or other object situation of third dimension degree, described thickness is considered to the ultimate range of short dimension, i.e. spherical or columniform diameter for example, and thickness range is with mentioned above identical.
c. basic weight
The basic weight of described personal care product and/or described dissolvable solid substrates calculates (g/m with selected personal care product and/or the described dissolvable solid substrates of the every area of weight of described personal care product and/or described dissolvable solid substrates 2).Described area calculates perpendicular to outer peripheral projected area at flat surfaces with described personal care product and/or described dissolvable solid substrates.With regard to flat articles, described area calculates according to the area surrounding in sample neighboring thus.With regard to spherical object, described area calculates according to average diameter thus, is 3.14 * (diameter/2) 2.With regard to cylindrical object, described area, according to average diameter and average length computation, is diameter * length thus.With regard to erose three-dimensional body, described area calculates according to this limit projecting to having on the flat surfaces of limit vertical orientation of maximum overall dimensions.
d. density of solid
The dissolvable solid substrates of personal care composition as herein described can be measured to characterize according to density of solid.
The density of solid of dissolvable solid substrates can be determined divided by the known volume of described solid by the weight of described solid.The volume of solid can be determined by many technology, be included in the described solid of the interior production of mould of known x-y size, and the thickness of measuring gained is to consider any contraction or expansion during drying process.Described solid also can be cut into known x-y size,, by using circular die or the square cutting punch die of known diameter or size, then passes through detect thickness.Alternatively, in the situation without any remarkable varied in thickness, described density can be calculated by following formula: the basic weight of bulk density=porosu solid/(porosu solid average thickness * 1,000) therein.
e. abscess interconnection degree
Personal care product of the present invention and/or dissolvable solid substrates have the abscess interconnection degree of height, are mainly perforate solid foams, rather than are mainly closed pore solid foam.Abscess interconnection degree can be evaluated by optical microscopy, scanning electron microscopy, micro-Computed tomography parameter (celestial body amasss and SMI index), gas survey proportion parameter (perforate %) or other suitable method.
The quantitative approach of measuring abscess interconnection degree is via optical microscopy.This can be by using shears or sharp blade, in the z-direction of measuring, cut wide rectangular of 2-3mm on described personal care product and/or described dissolvable solid substrates x-y maximum orthogonality surface, and the rectangular inside foam structure that turn 90 degrees to expose the transverse cross-sectional area of firm cutting of gained is carried out.Can pass through closely visual observation, or more accurate, by using and amplify as derived under the SZX12 stereoscopic microscope of Olympus Olympus America Inc. (Center Valley, PA) at stereoscopic microscope, evaluate this transverse cross-sectional area.Perforate personal care product of the present invention and/or dissolvable solid substrates are easy to identify by the interior section of inspection transverse cross-sectional area, described transverse cross-sectional area is mainly three-dimensional pillar network by comprising, comprise the third dimension along cross-sectional depth, described pillar has the unlimited void space of interconnection each other around.On the contrary, by being used to form the cutting process of the transverse cross-sectional area of exposure, the internal cross section of closed-cell foam will be rendered as the discrete bubbles being cut open, and only in the cross-sectional surface of bidimensional, interconnects.
The another kind of method of measuring abscess interconnection degree is and structural model index long-pending via celestial body.Use micro-computed tomography system (μ CT80, SN 06071200, Scanco Medical AG), the about 4cm of sweep diameter and high 3 to 7mm plate-like sample.Make the imaging when lying in cylindrical tube bottom of each sample.Image acquisition parameter is 45kVp, 177 μ A, 51.2mm visual field, 800ms integrating time, 1000 projections.Regulate number of leaves with Covering samples height.Data reconstruction group comprises great amount of images, and the pixel of each is 2048 * 2048, and isotropic imaging resolution is 25 μ m.With regard to data analysis, select to be positioned at completely the concerned volume of sample, avoid surf zone.Typical concerned volume is 1028 * 772 * 98 voxels.
Adopt the bone trabecula morphometry rating method of the Scanco Medical that threshold value is 17 to measure structural model index (SMI).With this index quantize bone trabecular structure outward appearance (referring to T.Hildebrand, the Quantification of bone microarchitecture with the structure model index.Comp Meth Biomech Biomed Eng of P.R ü egsegger 1997; The 1st volume: 15 to 23 pages).On orthogonal direction, minute quantity is stretched in trigonometric ratio surface, and calculate surface and the volume of area of new bone.Thus, can determine the difference quotient (dBS/dr) of bone surface.Then by following formulate SMI:
SMI = 6 · BV · dBS dr BS 2
SMI relates to the protruding rate of structure to types of models.The SMI that the plate of desirable (flat) has is 0 (it is unchanged that plate stretches lower surface), and the SMI that desirable cylindric bar has is 3 (bar stretches the linear increase of lower surface).The SMI that ball has is 4.Concave structure has negative dBS/dr, obtains negative SMI value.The artificial boundary of concerned volume edge is not included in calculating, therefore by its elimination.
Except Scanco Medical analyzes, also carry out star cubing.Celestial body is long-pending is the measuring of space space opening degree in two phase structure.By pay close attention to mutually in (under the situation at us, it is background) select random equally distributed series of points, we can with random direction from these point in each extend straight line.Described straight-line extension, until their contact prospect phases.Then record in these straight lines the length of each.In each direction, (x/y/z) gets 10 random some samples, and selects 10 random angles at each some place.If straight-line extension to the border of concerned ROI, discards described straight line (we only wish to accept and the mutually actual crossing straight line of prospect).The achievement in research of final formula based on announcing in " Star volume in bone research ", A histomorphometric analysis of trabecular bone structure using vertical sections; Vesterby, A.; Anat Rec.; In February, 1993; 235 (2) volumes: 325 to 334 pages.
Figure BDA0000066753880000221
Wherein " dist " is individual distance, and N is studied straight line number.
Via gas hydrometry, measure perforate percentage composition.Gas hydrometry is to use the common analytical technology of gas displacement method Accurate Measurement volume.Use noble gas if helium or nitrogen are as replacement media.Sample is sealed in the device compartment of known volume, imports suitable noble gas, be then expanded to another accurate internal volume.Measure the pressure before and after expanding, and for calculating sample volume.This volume, divided by sample weight, is drawn to gas displacement density.
ASTM standard method of test D2856 adopts older air contrast proportion instrument model, and the method for measuring perforate percentage ratio is provided.This device is no longer produced.Yet, by enforcement, adopting the test of the AccuPyc gravimeter of Micromeritics, you can facilitate and accurately measure perforate percentage ratio.ASTM method D2856 has described for measuring 5 kinds of methods (A, B, C, D and E) of foamed materials perforate percentage ratio.
With regard to these experiments, can, by using nitrogen and ASTM foampyc software, adopt Accupyc1340 to carry out analyzing samples.Method C in ASTM method is used for calculating perforate percentage ratio.The method compares with the true volume being recorded by Accupyc adopting thickness and normal volume to calculate the geometric volume recording simply.Recommendation is by Micromeretics Analytical Services, and Inc. (One Micromeritics Dr, Suite 200, Norcross, GA 30093) implements these mensuration.The more information that technology is relevant is therewith found in Micromeretics Analytical Services website (www.particletesting.com or www.micromeritics.com), or is published in the books " Analytical Methods in Fine particle Technology " of Clyde Orr and Paul Webb.
f. cell wall thickness
The cell wall thickness of described personal care product and/or described dissolvable solid substrates is calculated from scanogram by micro-computed tomography (CT) system (μ CT80, SN 06071200, Scanco Medical AG) as described herein.According to adopting the bone trabecula morphometry rating method of Scanco Medical to measure the determined method of bone trabecula thickness, measure cell wall thickness.As the bone trabecula thickness definition obtaining from Scanco User handbook: bone trabecula thickness is used Euclidean Distance Transform (EDM), described Euclidean Distance Transform calculate from any point of prospect to nearest background dot Euclidean distance.The twice of the center line value that the representative of bone trabecula thickness measurement is associated with EDM local maximum, the representative of EDM local maximum is apart from the distance (twice of this distance will obtain thickness) of object central authorities.
g. specific surface area
The specific surface area of described personal care product and/or described dissolvable solid substrates is measured by gas-adsorption technique.Surface area is the measuring of solid sample exposed surface of molecular level.BET (Brunauer, Emmet and Teller) theory is for measuring the Epidemic model of surface area, and it is based on Adsorption Isotherms.Gas absorption adopts physical absorption and capillary condensation to carry out mensurated gas composition adsorption isotherm.Described technology is summarized with the following step: sample is placed in to sample tube and under vacuum or mobile air heating to remove the pollution in described sample surface.By deduct the weight of sky sample tube from degassed sample+sample tube weight, obtain sample weight.Then sample tube is placed on to analysis port, and starts to analyze.The first step in analytical method is that sample tube is emptying, then under liquid nitrogen temperature, uses helium, measures the free space volumes of sample tube.Then sample is emptying for the second time, to remove helium.Then instrument quantitatively adds krypton-85 gas by the interval with user appointment, until reach required pressure, measures, and starts to gather adsorption isotherm.
Sample preparation (degassed): the sample that there is no fully to remove institute's adsorption fouling thing will be degassed during analyzing, and a part of surface will not be used to mensuration.Degassed object is before analysis, from sample surface, to remove the molecule of these absorption.Absorption molecule must arrive all parts on described surface, to represent real surface area.By heating described sample, simultaneously that sample tube is emptying, prepare sample.
With regard to these experiments, by sample emptying degassed spending the night at room temperature.Then can use ASAP2420 and Krypton absorption, analyzing samples.Krypton is more preferred than nitrogen, because its saturation pressure is approximately 1/300 (Krypton: 2.5 holders of atmosphere under liquid nitrogen temperature; Nitrogen: 760 holders).Therefore, compare with nitrogen, under same relative pressure, in the free space of sample top, have the nitrogen molecule of about Krypton molecular number 1/300.Because Krypton and the nitrogen molecule of the roughly the same number of needs forms monolayer, so this number represents in the ratio nitrogen situation of institute's addition large many.Can pass through Micromeretics Analytical Services, Inc. (One Micromeritics Dr, Suite 200, Norcross, GA 30093) implements these mensuration.The more information that technology is relevant is therewith found in Micromeretics Analytical Services website (www.particletesting.com or www.micromeritics.com), or is published in the books " Analytical Methods in Fine particle Technology " of Clyde Orr and Paul Webb.
h. the evaluation of surperficial resident coating
The existence of the resident coating in surface that the present invention comprises starch-spice complex can be determined by many technology.In order to detect granule or powder coating, the surface that dissolvable solid substrates applies and can checking by microscopic techniques perpendicular to the cross section on larger surface.These microscopic techniques can comprise optical microscopy and scanning electron microscopy (SEM).Described optical microscopy can comprise but must not be limited to bright territory, dark territory or confocal microscopic method technology.Other is for the independent element of mapping in cross-sectional surface, as silicon or distinctive functional group, as the technology of quaternary ammonium group comprises: flight time secondary ion mass spectrometry (ToF-SIMS) or infrared microscope method.
Be used for checking from described dissolvable solid substrates surface to internal particle distributing, and the possible method of described sample of not cutting into slices comprises: micro-computed tomography (CT) (micro--CT), NMR (Nuclear Magnetic Resonance)-imaging (MRI), acoustic imaging, confocal fluorescence microscopy method, confocal Raman spectra and confocal Infrared Reflective Spectra method.
The distribution that can cross by comparing granule the cross section of described porosu solid cutting of determining at the resident coating granule of dissolvable solid substrates cross section upper surface is carried out.Specifically, the cross section inside exposing by analyzing the solid of firm cutting, can determine that surperficial resident coating granule should be present on original consolidate/aerosphere face, rather than inner at the exposure cross section of solid cell wall.It should be pointed out that the cutting method due to porosu solid, may occur just some pollution of the solid cell wall cross section inside of cutting.Yet, described surface resident coating advantage distribution of particles (in one embodiment approximately 50% to approximately 100%) by occur in former solid/aerosphere face on rather than the cutting cross section that exposes in cell wall inner.
It should also be noted that the resident coating granule in surface of the present invention is generally non-uniformly distributed in the consolidate/gas interface of all exposures.On the contrary, find, the resident coating in surface of the present invention is conventionally according to gravity, is disseminated to approximately 0.5 to about 3.0mm in from coating application point to vestibule.Therefore, should, at a plurality of different tops to the bottom transverse cross section of porosu solid and edge to edge cross section, implement the mensuration (as mentioned above) of the resident granule in beautifying active substance of the present invention surface.If existed, the resident beautifying active substance granule in described surface is generally positioned near the surf zone (apart from described surface approximately 0.5 to about 3.0mm) that first applies coating.
i. spice panel of expert
Spice sensation panel of expert implements quantitative described fragrance performance in the shampoo rules scheme of standard, as mentioned below, with three expert's spice teachers with 1 to 100 evaluation of scale odor characteristics and odour intensity (abnormal smells from the patient that odorlessness extremely may be the strongest).The liquid shampoo product of retail is included in each group to (herbal essences shampoo is provided by Procter & Gamble) in contrast.
The evaluation of described spice panel of expert " is carried out on the original toupees of straight Asians at 15g/10.With shower nozzle, with 100 °F of tap waters, with 1.5 to 2.0 gallon per minute, rinse and describedly to send out bunches 20 seconds.In order to test described liquid reference product, first described liquid heard the abnormal smells from the patient of net product in the glass jar of an opening.Then by 5cm 3fluid product be administered on the palm of moistening in advance for evaluating the strong degree of initial spice on hand.Next, with palm, liquid application bunch is bubbled 40 seconds to the central authorities of described bunch and by moving downward with two handss repeatedly to rub and push described sending out, for sending out bunch the evaluation of foam abnormal smells from the patient.Then by described bunch cleaning down 45 seconds and evaluate the abnormal smells from the patient of moistening hair.Additional evaluation comprises 4 hours moist hair abnormal smells from the patients, 24 hours dry hair abnormal smells from the patients and 24 hours rewetting abnormal smells from the patients.
When test solubility porosu solid of the present invention, by the substrate (about 1.0 to 1.1 grams) of shim form, substitute 5cm 3liquid.In order to measure solubility porosu solid, first described pad is heard in the big envelope of opening recently, for the abnormal smells from the patient of net product.Then described pad is administered on the palm of moistening in advance, and with the tap water dilution of 100 °F of 7.5ml, along with palm friction (4 to 8 strokes) until described solid dissolve completely, in the initial strong degree evaluation of spice on hand.Next, with palm, the liquid mixture of gained be administered to the described central authorities of sending out bunch and bunch bubble 40 seconds by moving downward with two handss repeatedly to rub and push described sending out, for sending out bunch the evaluation of foam abnormal smells from the patient.Then as mentioned above, by described bunch cleaning down 45 seconds and evaluate moistening hair abnormal smells from the patient, 4 hours moist hair abnormal smells from the patients, 24 hours dry hair abnormal smells from the patients and 24 hours rewetting abnormal smells from the patients.
IV. using method
Compositions of the present invention can be used for processing mammalian keratinous tissue as hair and/or scalp, and provides and can get performance express developed.For nursing one's health the method for described hair, can comprise the following steps: a) use the described personal care product of effective dose to hand, b) with personal care product described in water-wet, also rub to dissolve described solid, c) material of using dissolving is to be processed as hair or scalp, and d) water rinses also dilution process agent from hair or scalp.These steps can repeat many times on demand, to reach desired processing beneficial effect.
V. embodiment
Following examples have further described with illustration the embodiment in protection domain of the present invention.These given embodiment are only illustrative, unintelligible for being limitation of the present invention, because can make many modification under the condition that does not deviate from essence of the present invention and scope.Except as otherwise noted, the amount of all examples is by the concentration of the weighing scale of total composition, that is, and and wt/wt percentage ratio.
embodiment 1: prepare dissolvable solid substrates
The percentage by weight preparation of following Surfactant/Polymer liquid processing compositions to indicate, described in following table 1.
table 1
Figure BDA0000066753880000261
1Sigma-Aldrich Catalog Sequence Number 363081, MW 85,000 to 124,000,87-89% hydrolysis
2McIntyre Group Ltd,University Park,IL,Mackam HPL-28ULS
3UCARE tMpolymer LR-400, derives from Amerchol Corporation (Plaquemine, Louisiana)
By use conventional overhead stirrer (
Figure BDA0000066753880000262
rW20DZM Stirrer, derives from
Figure BDA0000066753880000263
works, Inc., Wilmington, DE) and hot plate (Corning Incorporated Life Sciences, Lowell, MA) prepare the above-mentioned composition of 300 grams of target weights.In suitable big or small and clean vessel, under 100 to 150rpm stirrings, add distilled water and glycerol.When existing, then under constant stirring, slowly add cationic polymer until evenly.In suitable container, weigh polyvinyl alcohol, and use spoon slowly to join in main mixture with little increment, continue to stir, to avoid forming obvious agglomerate simultaneously.Regulate mixing speed so that formation of foam minimizes.Mixture is slowly heated to, after 80 ℃, add surfactant.Then described mixture is heated to 85 ℃, continues to stir simultaneously, then make it be cooled to room temperature.Add additional distilled water with the water (based on the initial tare weight of container) of compensate for evaporation loss.Final pH, during 5.2 to 6.6, if needed, and regulates with citric acid or dilute sodium hydroxide.Measure the process mixture viscosity of gained.
Dissolvable solid substrates (in this paper embodiment also referred to as " substrate ") is described in table 2 below by aforesaid liquid process mixture and prepares.
table 2
Inflationtime (second) 62
Moistening density (g/cm 3) 0.26
Furnace temperature (℃) 130
Drying time (minute) 38
Dry matrices average weight (g) 1.10
Dry matrices average thickness (cm) 0.62
Substrate average shrinkage (%) 4.6%
Dry matrices average density (g/cm 3) 0.11
Average basis weight (g/m 2) 650
At 70 ℃, the process mixture of 300 grams (deriving from embodiment 1) is stored in convection furnace and surpasses two hours to preheat described process mixture.Then described mixture is transferred to and is preheated
Figure BDA0000066753880000271
mixer Model K5SS (derives from Hobart Corporation, Troy, OH) the rustless steel bowl of 5 quarts (by being placed in 70 ℃ of stoves over 15 minutes), described bowl outfit flat beater connector and the water-bath connector that comprises 70 to 75 ℃ of tap waters.Described mixture is acutely inflated to be set to 10 maximum rate, until obtain about 0.26 gram/cm 3the described density of moistening density (time is recorded in table) by weighing, there is the cup being full of of known volume and with scraper, flatly scrape the top of wiping cup and measure.Then the mixture that filled gas of gained is spread out in the aluminum die of square 160mm * 160mm with scraper, described mould has the 6.5mm degree of depth, with 45° angle, hold large metallic spatula, with the slowly even floor mop of its straight flange, cross described die surface by excessive moistening suds removal.Then described aluminum die is placed in to about 35 to 45 minutes of the convection furnace of 130 ℃.Make described mold cools down to room temperature, under the help of thin scraper and tweezers, dry substantially dissolvable solid substrates is removed from mould.
(each square has about 16.9cm to use cutting punch die and Samco SB20 cutting machine that the 160mm of each gained * 160mm square substrate is cut into nine 43mm * 43mm square (having circular edge) 2surface area).Then by the less substrate of gained in being open to the large valve bag of room air, remaining on 70 °F and the indoor equilibrate overnight of 50% relative humidity constant environment (14 hours).Then each substrate of weighing is also positioned over initial mould one side downwards independently in weighing ware.Record substrate average weight and described basic weight and pass through substrate average weight divided by 0.00169 square metre of calculating.The stromal thickness of gained is measured and record with digital caliper.Described valve bag seals in 50% relative humidity environment.
embodiment 2: the structural characterization of dissolvable solid substrates
Following table 3 has been summarized structure measurement and the physical integrity classification qualitatively of obtaining from the dissolvable solid substrates of embodiment 1.Also obtain compared with the SEM of low-density goods and micro--CT image and be referenced in the figure of appendix.Data method record as described herein.
table 3
Figure BDA0000066753880000281
Above-mentioned data and reference picture are shown that the dissolvable solid substrates described in embodiment 1 is mainly perforate and are had a good physical integrity.Correspondingly, the dissolvable solid substrates that is mainly perforate also shows quick solubility property (6 to 8 strokes) artificial hand as described herein in dissolving rules.
comparing embodiment 3: the dissolvable solid substrates shampoo of the second spice 2a that contains spice 1a and surface-coated beta-schardinger dextrin-complex
The dissolvable solid substrates shampoo " substrate " (with corresponding tared dish) that derives from embodiment 1 is removed and taring to 0% weight on 4 grades of weight balances the plastic bag from sealing.In ventilated chamber, described substrate is arranged on the angle of approximately 60 degree and is placed on stainless steel frame, described shelf has indenture support matrix to be prevented from gliding, and has a hole at plate, so that described substrate can be by pushing away easily and remove from support from base plate.Importantly, the top surface of described substrate (in drying oven, be exposed to air that side and with during drying process, directly that side of the described aluminum die of contact is contrary) away from described shelf.Vial with pump spray is filled with the first perfumery oil 1a, and then the distance of from 2 to 3 inches is ejected into the surface of described substrate.Then described substrate is removed and put back to the tared dish on balance from shelf, make one side, top outside.The weight of the spice that record applies, and in the situation that target weight does not reach, or apply emitted dose another time, or from described substrate, sponge excessive spice with Kim cleaning piece.Repeat this iterative process until reach described target weight scope.The amount of the spice 1a that record applies in following table.The substrate that leans against gained on little tared dish is stored in valve bag and the isolated air of sealing.To deriving from second substrate of embodiment 1, repeat above-mentioned technique.
Next described the first substrate in its tared dish removed from valve bag, and on 4 grades of weight balances taring to 0% weight again.Then the high spice accord 2a beta-schardinger dextrin-complex that affects of the second spice (is pressed to described inclusion complex weighing scale, it is compound with 8.50% that height affects spice accord, and according to the exercise question of being submitted on May 19th, 2005 by people such as Deckner, be the patent application of " Oil Encapsulation ", by spray drying process, prepare) be administered to the surface of each substrate.Then by described spice inclusion complex powder coated for substrate, by in wiggly mode, on the plate that comprises excessive described spice inclusion complex, (or other suitable container) shakes described substrate ten times (described technique is repeated in other side) lightly.Then the substrate of the powder coated of gained is taken up to (with the hands of glove) and shake lightly and tip-tap several times to remove any excessive powder in described substrate that fully do not adhere to.The weight record that the second spice height is affected to spice accord 2a beta-schardinger dextrin-composite coated gained is in following table.Then in the porous matrix in its tared dish being put back into valve bag, also sealing completely cuts off air.For the second substrate, repeat this power applications technique.
During the final weight obtaining is provided in the following table.
embodiment 4: the dissolvable solid substrates shampoo with spice 1a and surface-coated calcium silicates class complex the second spice 2a
Flacktek Speemixer is used in the preparation of the inorganic particulate perfume complex of the present invention's (comprising calcium silicates class) the second spice 2a tMdAC400FV (By HAUSCHILD, Waterkamp 1,509075Hamm, Germany) and fourth gear weight balance are made.By the calcium silicates class of 5 grams (Hubersorb 600, by Huber Engineered Materials, Havre de Grace, MD provides, and by the oil that supplier report has a 475cc/100g, is absorbed the particle mean size of 6 microns, 300m 2the BET surface area of/g and the bulk density of 8lbs/CFT) weigh to the wide mouthed bottle of Flacktek Speedmixer maximum 60.Then use pipet that the described second perfumery oil 2a of 5 grams is weighed to the wide mouthed bottle of identical maximum 60.Then described wide mouthed bottle is covered with corresponding bottle cap airtight, and under 2750rpm about 60 seconds of mixed at high speed.Therefore described height affects spice accord 2a by described complex weighing scale, and with about 50% compound, and the complex of gained is the form of free-flow fine powder.
Dissolvable solid substrates shampoo, according to identical as described in Example 3 formula and operation preparation, still substitutes the second spice 2a beta-schardinger dextrin-complex with described the second spice 2a calcium silicates class complex.During the final weight obtaining is provided in the following table.
Figure BDA0000066753880000301
embodiment 5: the dissolvable solid substrates shampoo with spice 1b and surface-coated calcium silicates class complex the second spice 2b
The preparation of the second spice 2b calcium silicates class complex is made by calcium silicates class with method as identical in embodiment 4, but substitutes the second spice 2a with the second spice 2b.By described complex weighing scale, described height affects spice accord 2b so with about 50% compound, and the complex of the gained form that is free-pouring fine powder.
Dissolvable solid substrates, according to identical as described in Example 3 formula and operation preparation, still substitutes spice 1a with different spice 1b, and substitutes the second spice 2a beta-schardinger dextrin-complex with described the second spice 2b calcium silicates class complex.During the final weight obtaining is provided in the following table.
Figure BDA0000066753880000302
Figure BDA0000066753880000311
embodiment 6: the dissolvable solid substrates shampoo with the second spice 2c of spice 1c and surface-coated calcium silicates class complex
The preparation of the second spice 2c calcium silicates class complex is made by calcium silicates class with method as identical in embodiment 4, but substitutes the second spice 2a with the second spice 2c.By described complex weighing scale, described height affects spice accord 2c so with about 50% compound, and the complex of the gained form that is free-pouring fine powder.
Dissolvable solid substrates, according to identical as described in Example 3 formula and operation preparation, still substitutes spice 1a with different spice 1c, and substitutes the second spice 2c beta-schardinger dextrin-complex with described the second spice 2a calcium silicates class complex.During the final weight obtaining is provided in the following table.
embodiment 7: the dissolvable solid substrates shampoo with spice 1c and surface-coated calcium silicates class complex the second spice 2b
The second spice 2b calcium silicates class complex is as prepared equally at embodiment 5 second spice 2b calcium silicates class complex.
Dissolvable solid substrates according to as at embodiment 5 described in same recipe and operation preparation, but with the alternative spice 1b of different spice 1c.During the final weight obtaining is provided in the following table.
Figure BDA0000066753880000321
embodiment 8: the dissolvable solid substrates shampoo of the second spice 2d that contains surface-coated silica shell complex
The second spice 2d silica shell complex derives from Kobo Inc. (690Montrose Ave., South Plainfield NJ 07080) with code SSl3M.Described height affects spice accord 2dYou supplier report by described complex weighing scale, and with about 75% compound, and the complex of gained is free-pouring fine powder form.
Dissolvable solid substrates, according to identical as described in Example 3 formula and operation preparation, does not still have spice 1a, and substitutes the second spice 2a beta-schardinger dextrin-complex with described the second spice 2d silica shell complex.During the final weight obtaining is provided in the following table.
Figure BDA0000066753880000331
spice sensation panel of expert evaluates
Following table has been summarized the data of spice sensation panel of expert, will be described in the dissolvable solid substrates shampoo that comprises spice 1a and the second spice 2a calcium silicates class complex in embodiment 3 and 4 and the dissolvable solid substrates shampoo comparison that comprises spice 1a and the second spice 2a beta-schardinger dextrin-complex.Data are collected by method as described herein.
intensity scale 1 to 100 (odorlessness extremely may be the strongest)
Figure BDA0000066753880000332
Figure BDA0000066753880000341
Above-mentioned data display is with respect to shampoo liquid tester, for beta-schardinger dextrin-complex and calcium silicates class complex (initial dissolution and completely dilution), described dissolvable solid substrates is when being dissolved in the water, significantly and the appreciable perfume delivery of panel of expert.In addition, at moistening, 6 hours and 24 hours point, with respect to described liquid shampoo tester, feel that the spice of gained is stronger to the persistency hair from the substrate of preparing with two kinds of spice complex, and observe with respect to described beta-schardinger dextrin-complex, for described calcium silicates class complex, there is directed improvement.Above-mentioned data display can be obtained with respect to the similar performance of molecule inclusion coordination compound (beta cyclodextrin) by inorganic particle of the present invention (calcium silicates class)-spice complex.
Following table has been summarized spice sensation panel of expert data, relatively as being described in the dissolvable solid substrates shampoo of the calcium silicates class complex that comprises the first different spice and different the second spice in embodiment 5,6 & 7.Method collection as described herein for described data.
intensity scale 1 to 100 (odorlessness extremely may be the strongest)
Figure BDA0000066753880000342
Figure BDA0000066753880000361
Above-mentioned data display is with respect to described shampoo liquid tester, significantly and the perfume delivery of the appreciable substrate of panel of expert, prepared by the calcium silicates class complex of the combination of two kinds of second different spice and first spice different from two kinds for described substrate (initial dissolution and dilute completely).In addition,, at moistening, 6 hours and 24 hours point, with respect to described liquid shampoo tester, feel that the spice of gained is stronger to the persistency hair from the substrate of preparing with calcium silicates class complex.The motility of above-mentioned data display the present invention surface resident inorganic particle (calcium silicates class)-spice complex.
Following table has been summarized spice sensation panel of expert about as described in Example 8, the data of the solubility porosu solid shampoo that comprises the second spice silica shell complex.Described data are collected by method as described herein.
intensity scale 1 to 100 (odorlessness extremely may be the strongest)
Figure BDA0000066753880000362
Above-mentioned data display is at 4 hours and 24 hours point, with respect to described liquid shampoo tester, from the dissolvable solid substrates shampoo of the second spice of the silica composite that comprises surface-coated to hair the improvement of spice persistency orientation.The effect of inorganic particle (silica shell)-spice complex that above-mentioned data display the present invention is different, does not even have the first spice.
Notice, any active substance disclosed herein and/or compositions can be used for goods and/or use together with goods, and specifically, care and household goods, described goods are disclosed in the application of following United States Patent (USP) publication, comprise that requirement is to the wherein priority of any announcement: US 61/229981, US61/229986, US 61/229990, US 61/229996, US 61/230000 and US 61/230004.This based article can comprise one or more following components: detersive surfactant, plasticizer, enzyme, foam inhibitor, short infusion, bleach, bleaching stibilizer, chelating agen, cleaning solvent, hydrotropic agent, divalent ion, fabric-softening agent addition agent (as quaternary ammonium compound), non-ionic surface active agent, spice and/or perfume delivery systems.This based article can be used in method, and described method includes but not limited to: quantitatively add washing machine to clean and/or to process fabric; Quantitatively add dish-washing machine to clean and/or to process tableware; Quantitatively be added to the water to clean and/or process fabric and/or hard surface.
The relevant part of all references is incorporated herein by reference, and quoting of any document may not be interpreted as approval as prior art of the present invention to it.
Although illustrated and described the present invention by specific embodiments, it will be apparent to those skilled in the art that and in the situation that not deviating from the spirit and scope of the invention, can make many other change and modification.Therefore, at additional claims, comprise all these changes and the modification in the scope of the invention consciously.

Claims (17)

1. a personal care product, described goods comprise:
A.) dissolvable solid substrates, described substrate comprises:
I. account for 10% to 75% surfactant of described personal care product weight;
Ii. account for 10% to 50% water-soluble polymer of described dissolvable solid substrates weight;
Iii. account for 1% to 30% plasticizer of described dissolvable solid substrates weight;
Wherein said dissolvable solid substrates has 80% to 100.0% perforate percentage composition, and
B.) surperficial resident coating, described coating comprises one or more inorganic particulate perfume complex of 10% to 100%;
Wherein said inorganic particulate perfume complex refers to that spice is compounded in the releasable substrate of the water consisting of particle form inorganic material, wherein the ratio at inorganic particle described in described complex and spice is 0.5:1 to 19:1, and the ratio of the resident coating of wherein said dissolvable solid substrates and described surface is 110:1 to 0.5:1
Wherein said inorganic particulate perfume complex comprises inorganic material, described inorganic material choosing is the group of following composition freely: silicate, carbonate and their combination, wherein said silicate and carbonate form by carbonate or silicate and metal reaction, described metal choosing is the group of following composition freely: alkali (IA) metal, alkaline earth (IIA) metal and transition metal
The ratio of the resident coating of wherein said dissolvable solid substrates and described surface is 20:1 to 1:1,
The inorganic particle that wherein said complex comprises 0.7:1 to 6:1 ratio and spice,
Wherein said dissolvable solid substrates has 125g/m 2to 3,000g/m 2basic weight, and the thickness of 0.5mm to 10mm, and wherein said dissolvable solid substrates comprises 0.03m 2/ gram to 0.25m 2/ gram specific surface area, and wherein said dissolvable solid substrates has 80% to 100.0% perforate percentage composition, and wherein said dissolvable solid substrates has the cell wall thickness of 0.02mm to 0.15mm.
2. personal care product as claimed in claim 1, wherein said inorganic particulate perfume complex is included as the inorganic material of synthetic calcium silicate.
3. personal care product as claimed in claim 1, wherein said surfactant comprises at least one I class surfactant, wherein said I class surfactant is anion surfactant, described anion surfactant choosing is the group of following composition freely: alkyl sulfate and alkyl ether sulfate, Sulfated monoglyceride, the alkene of sulfonation, alkylaryl sulfonates, uncle or secondary alkyl sulfonate, alkyl sulfosuccinate, acid taurate, acid isethionate, alkyl glycerol ether sulfonate, sulfonation methyl ester, alpha-sulfonated fatty acid, alkylphosphonic, acyl glutamate, acyl sarcosinates, alkyl lactate, anionic fluorosurfactants, and their combination.
4. personal care product as claimed in claim 3, wherein said surfactant is sodium lauroyl glutamate.
5. personal care product as claimed in claim 1, wherein said surfactant also comprises II class surfactant, wherein said II class surfactant choosing is the group of following composition freely: both sexes, zwitterionic and their combination.
6. personal care product as claimed in claim 1, wherein said surfactant choosing is the group of following composition freely: the surfactant of 0.1% to 10% ionic surface active agent, non-ionic surface active agent, polymerization and their any combination.
7. personal care product as claimed in claim 1, the ratio of the resident coating of wherein said dissolvable solid substrates and described surface is 10:1 to 1.5:1.
8. personal care product as claimed in claim 7, the ratio of the resident coating of wherein said dissolvable solid substrates and described surface is 7:1 to 3:1.
9. personal care product as claimed in claim 1, the resident coating in surface that wherein comprises described inorganic particulate perfume complex is powder.
10. personal care product as claimed in claim 1, the resident coating in surface that wherein comprises described inorganic particulate perfume complex is linked at least a portion of the outer surface of described dissolvable solid substrates.
11. personal care products as claimed in claim 1, wherein said solubility personal care product comprises two dissolvable solid substrates, and the resident coating in surface that wherein comprises described inorganic particulate perfume complex is the layer between described two dissolvable solid substrates.
12. personal care products as claimed in claim 1, the inorganic particle that wherein said complex comprises 1.1:1 to 3:1 ratio and spice.
13. 1 kinds of methods for the manufacture of personal care product as claimed in claim 1,
Described goods comprise:
A.) dissolvable solid substrates, described substrate comprises:
I. account for 10% to 75% surfactant of described personal care product weight;
Ii. account for 10% to 50% water-soluble polymer of described dissolvable solid substrates weight;
Iii. account for 1% to 30% plasticizer of described dissolvable solid substrates weight;
Wherein said dissolvable solid substrates has 80% to 100.0% perforate percentage composition, and
B.) surperficial resident coating, described coating comprises one or more inorganic particulate perfume complex of 10% to 100%;
Wherein said inorganic particulate perfume complex refers to that spice is compounded in the releasable substrate of the water consisting of particle form inorganic material, wherein the ratio at inorganic particle described in described complex and spice is 0.5:1 to 19:1, and the ratio of the resident coating of wherein said dissolvable solid substrates and described surface is 110:1 to 0.5:1
Wherein said inorganic particulate perfume complex comprises inorganic material, described inorganic material choosing is the group of following composition freely: silicate, carbonate and their combination, wherein said silicate and carbonate form by carbonate or silicate and metal reaction, described metal choosing is the group of following composition freely: alkali (IA) metal, alkaline earth (IIA) metal and transition metal
The ratio of the resident coating of wherein said dissolvable solid substrates and described surface is 20:1 to 1:1,
The inorganic particle that wherein said complex comprises 0.7:1 to 6:1 ratio and spice,
Wherein said dissolvable solid substrates has 125g/m 2to 3,000g/m 2basic weight, and the thickness of 0.5mm to 10mm, and wherein said dissolvable solid substrates comprises 0.03m 2/ gram to 0.25m 2/ gram specific surface area, and wherein said dissolvable solid substrates has 80% to 100.0% perforate percentage composition, and wherein said dissolvable solid substrates has the cell wall thickness of 0.02mm to 0.15mm;
Described method comprises:
(a) prepare process mixture, described mixture comprises 10% to 75% described surfactant, 10% to 50% described water-soluble polymer and 1% to 30% described plasticizer;
(b) by gas being incorporated in process mixture, inflate described process mixture to form the wet mix of filling gas;
(c) the described wet mixture that makes to fill gas forms one or more desired shapes;
(d) wet mix of filling gas described in dry is to form described dissolvable solid substrates; And
(e) the resident coating in surface that comprises powder type inorganic particulate perfume complex described in using is to described dissolvable solid substrates.
14. methods as claimed in claim 13, the wherein said resident coating in described surface that comprises described inorganic particulate perfume complex is administered on described dissolvable solid substrates with 20% to 70% humidity.
15. methods as claimed in claim 13, the wherein said resident coating in described surface that comprises described inorganic particulate perfume complex is administered on described dissolvable solid substrates with 30% to 60% humidity.
16. methods as claimed in claim 13, the wherein said resident coating in described surface that comprises described inorganic particulate perfume complex is administered on described dissolvable solid substrates with 5% to 20% humidity.
17. methods as claimed in claim 16, the wherein said resident coating in described surface that comprises described inorganic particulate perfume complex is administered on described dissolvable solid substrates with 7% to 15% humidity.
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